Process of making yellow basic dyes.



UNITED STATES PATENT Fries.

PAUL JULIUS AND WALTHER REESS, OF LUDWIGSIIAFEN, GERMANY, ASSIGN- ORS TOTHE BADISCHE ANILIN AND SODA FABRIK, OF SAME PLACE.

PROCESS OF MAKING SPECIFICATION forming part of Letters Patent No.644,324, dated February 27,1900.

Application filed september l, 1899.

To all whom it may concern.-

Be it known that we, PAUL JULIUS, doctor of philosophy, a subject of theEmperor of Austria-Hungary, and WALTHER REESS, doctor of philosophy, asubject of the King of Bavaria,residing at LudWigshafen-on-the-Bhine, inthe Kingdom of Bavaria and Empire of Germany, have invented new anduseful Improvements in Processes of Manufacturing Yellow BasicColoring-Matter, of which the following is a specification.

Our invention relates to an improvement in the art of manufacturingyellow basic coloring-matter.

In United States Letters Patent No. 637, 183, of November 14, 1899,there has been described a process of making a new yellow basiccoloring-matter by treating diamidotoluyl alcohol with beta-naphthylaminand beta-naphthylamin hydrochlorid. This diamido-toluyl alcohol wasfirst obtained by Terrisse and Darier, as described in the abovenamedLetters Patent, from meta-toluylenediamin and one molecular proportionof formaldehyde by mixing these bodies together in aqueous solution atthe ordinary temperature. Now we have found that the same productresults if the diamido-toluyl alcohol above referred to be treated withbeta-naphthol in the presence of an oxidizing agent, such as ferricchlorid.

The following example will show how our invention can best be carriedout. The parts are by weight.

Example: Ninety-five parts of diamidotoluyl alcohol and one hundred andthirty parts of crystallized ferric chlorid are mixed and reduced to afine powder. This powder is then introduced intoone hundred and fiftyparts of molten beta-naphthol Serial No. 729,186. (No specimens.)

at a temperature of 1A0 centigrade and contained in an enameled vessel.Now raise the temperature to about 150 to centigrade (one hundred andfifty to one hundred and seventy degrees centigrade) and maintain it sofor about two (2) hours, stirring the mass in the meanwhile. The meltdarkens and becomes viscous. Cool and powder the melt and extract thecoloring-matter from it by means of about fifteen thousand (15,000)parts of boiling water. Filter from the resinous byproducts, audprecipitate the coloring-matter from the filtrate by means of commonsalt.

If it be desired to obtain the coloring-matier quite pure, dissolve thehydrochlorid as precipitated by common salt in water, precipitate thecoloring-matter base from it by means of sodium carbonate, recrystallizethe base from toluene, and convert the purified base into itshydrochlorid by means of hydrochloric acid.

Now we claim 1. The improvement in the art of manufacturing basic yellowcoloringmatter which consists in treating diamido-toluyl alcohol withbeta-naphthol and an oxidizing agent, all substantially as described.

2. The-improvement in theart of manufacturing basic yellowcoloringmatter which consists in treating diamido-toluyl alcohol withbeta-naphthol and ferric chlorid, all substantially as described.

In testimony whereof we have hereunto set our hands in the presence oftwo subscribing witnesses.

PAUL JULIUS. WALTHER REESS. Witnesses: I

BERNHARD O. HEssE, HOWARD E. J. INGLEY.

